SU732364A1 - Method of producing synthetic lubricating oil - Google Patents

Description

The invention relates to petroleum MJIH, in particular to a method for producing a lubricating oil based on copolymers of ethylene with propylene, having a high viscosity index and a low pour point. Synthetic lubricating oil can be used both independently and in a mixture with petroleum oils, improving their physico-chemical properties. and operational properties. A method of producing synthetic oils is known by contacting a mixture containing ethylene and propylene with a Ziegler catalyst to obtain a molecular weight copolymer of 5,000-900,000. The copolymer is then decomposed in the presence of a catalyst at 315–590 ° C to obtain lubricating oil 1. A disadvantage of this method is the necessity of using an expensive elution catalyst at the decomposition stage of an aluminosilicate zeolite promoted with oxides of rare earths. There is also known a method for producing synthetic lubricating oil by polymerizing ethylene with propylene to obtain a product with a molecular weight of 900-4000 and then thermally decomposing it to lubricating oil 2. This method is characterized by the following features. The copolymerization of ethylene with propylene is carried out in the liquid phase at a temperature from 0 to 125 ° C in the presence of a catalytic system consisting of a transition metal compound and gshyumini alkyl halide (Ziegler-Natta type catalyst). The ratio of monomers in the reaction zone is maintained so as to obtain a copolymer of a given composition containing from 29 to 71 mol.% Of ethylene, the rest is propylene. The efficiency of the catalyst is 150375 g of copolymer per 1 g of catalyst. The process proceeds at a hydrogen partial pressure of 1.4 to 140 kg / cm, which is high enough to produce a copolymer with a maximum average chiol molecular weight of about 4000.

To obtain oils of the required viscosity, the copolymers are thermally decomposed under reduced pressure, for example in a vacuum reactor, at a temperature of 350-450 C and a pressure of 0.1-5.0 mm Hg.

The disadvantage of this method of producing synthetic lubricating oil is the need to use hydrogen in the polymerization stage to reduce the molecular weight of the copolymer. In addition, the introduction of hydrogen into the reaction system leads, in turn, to a decrease in the process rate, a higher specific catalyst consumption (since the yield of the target product per unit of catalyst weight decreases) t to the necessity of washing and removing the catalyst from the resulting copolymer and reducing the efficiency of the process generally.

The aim of the invention is to increase the yield of the target product and increase the efficiency of the process.

The goal is achieved in that in the process of producing synthetic lubricating oil by copolymerizing ethylene with propylene on a Ziegler-Natta type catalyst system followed by thermal decomposition of the obtained copolymer, the copolymerization is carried out to obtain a copolymer with a molecular weight of 100,000-1,000,000.

Copolymerization can be carried out to obtain a copolymer containing 40-85 mol. % ethylene.

Thermal decomposition is preferably carried out at a temperature of 385-42 and a pressure of 10-300 mm Hg.

Ethylene copolymerization with propylene is carried out in liquid propylene under the temperature and pressure of 5-20 kg / cm metallOOPganicheskogo in the presence of a catalyst representative of a vanadium triacetylacetonate (AszU) -diizobutilalyuminyyhlorid (Diebach) or D & E-gilalyuminiyhlorid trihloroksivanady either () or diethylaluminum -diizobutilalyuminiyhlorid .

The ratio of monomers in the reaction zone is maintained so as to obtain a copolymer containing 40-85 Mdn.% Of ethylene. The process proceeds in the absence of hydrogen, and a solid copolymer with a molecular weight of 100000-1dOOOOQ is formed. The effectiveness of the catalyst is 4000-16000 g of the copolymer per 1 g of catalyst.

To obtain an oil of the required viscosity, the copolymer obtained without pretreatment is subjected to thermal decomposition under vacuum at a temperature of 385-430 ° C and a residual pressure of 10-30 O, preferably 10-80 mm Hg. The decomposition products are dispersed in vacuo with the release of

oil fraction boiling above (in terms of atmospheric pressure).

The resulting oil has high physicochemical properties, a low pour point and a high viscosity index.

The process of obtaining oil can be carried out both periodically and continuously.

Example. In a dry reactor and stainless steel with a volume of 7 liters, equipped with a non-contact stirrer, 5 liters of liquid propylene are fed and then saturated with ethylene until the pressure in the reactor reaches 5.7 kgf / cm, which corresponds to an ethylene content in the liquid phase of 4 mol%. Experience conduct: P1zh. After creating the process conditions, first 0.60 g of cocatalyst —DIVAH — is introduced into the reactor, and then 0.15 g of catalyst —. The ratio of A: V support is equal to 8: 1. The process is carried out in a liquid propylene medium. The catalyst and cocatalyst are introduced into the reaction zone as a solution in benzene and gasoline, respectively, at a concentration of 1-3%. The time of the experiment is 40 min. After this time, the stirrer is stopped, the pressure in the reactor is released, the reaction mass is dried and further subjected to thermal decomposition. The ethylene-propylene copolymer obtained is as follows:

The content of propylene in the copolymer, mol%. 50 intrinsic viscosity, dl / g3,6

Molecular weight 331100 Copolymer yield, g 600 Copolymer yield g / g AcjV4000

Due to the high copolymer yield per g of catalyst, it is not necessary to wash it off from the catalyst. 600 g of the obtained copolymer is loaded into a thermal decomposition reactor, which is carried out at a temperature of 415 s and a residual pressure of 20 mm Hg. and continue until the high molecular weight ethylene-propylene copolymer is completely converted into a liquid product. 60-100 minutes is sufficient for this. Temperature and residual pressure are maintained constant throughout the experiment with the help of corresponding regulators.

The oil obtained as a result of the decomposition of the ethylene-propylene copolymer is characterized by the following parameters (without hydrogenation): & liquid product flow, g575 Copolymer yield, g / g

3833

Acjv

Kinematic viscosity at, cSt

3.02

170

Viscosity index The temperature is solidified according to the procedure described in Example 1. The content of ethylene is

The obtained samples of the copolymer of different composition is subjected to thermal decomposition at a temperature and residual pressure

20 mmHg The properties of the resulting. | With the decomposition of oils are given in Table. 2, where for comparison are given

35 also properties of the oil on prototype 2

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Examples 10-14. TepMHJecKoe decomposition of a copolymer containing 48 mol.% Of propylene and 52 mol.% Of ethylene is carried out at a temperature

Pr-merysy 15-17. The copolymer containing 42 mol.% Of propylene and 58 mol.% Of ethylene is thermally decomposed, changing the decomposition temperature from 385 to 425 C. Decomposition

Example 18. This example describes the technological scheme, illustrating the continuous implementation of the process (see drawing).

In the polymerization reactor 1, equipped with a mixing device and a thermostatic jacket, serves

 and various residual pressures

The results are shown in Table. 3

Table

carried out at a residual pressure of 40 mm Hg.

The quality of the oil obtained at different temperatures is given in t abl. four.

Table

the following components: UOSVZ catalyst and cocatalyst - DIBAH in a ratio of 1: 3 in the form of a 3-10% (by weight) solution in gasoline in the amount of 8-10 g / h, propylene and ethylene in quantities that provide the specified reactor performance

Claims (3)

Claim 1. The method of producing synthetic lubricating oil by copolymerization of Ethylene with propylene in the presence of 25 Ziegler-Natta catalyst, followed by Thermal decomposition of the resulting copolymer, with the exception of a rout and the fact that, in order to increase the yield of the target product and. 30 process efficiency, the copolymerization is carried out to obtain a copolymer with a molecular weight of 100000-1000000. 2. The method of pop. 1, characterized in that the copolymerization 35-lead to obtain a copolymer containing 40-85 mol.% Ethylene. 3. The method according to PP. 1 and 2, on t l with I ichayuschy in that the thermal decomposition is carried out at temperatures _n round 385-425 ° C and a pressure of 10-300 mm Hg ⁴⁰